Production of montan wax



Patented A r. 8. 1930 1,753,816

UNITED STATES PATENT OFF-ICE rnr'rz zscnocnum: HERBERT Bonnier, orumrzanonmoim, 0mm, ASSIGN- ons To a. nmancxscnn moxunwnaxnaxrmnensnuscmr, or BALI-E, man, (mam! raonu'c'rron or MONTAN wax" NoDrawing. Application filed larch 13, 1928, Serlal No. 281,406,

- This invention relates to the production of Montan wax. This productas hitherto obtained by extracting bituminous coal, especiallybrown-coal, with organic solvents is of a dark-brown to black colorwhereby the possibilities of utilizing the product are lessened I ertyis peculiar to certain oxy enated to a considerable extent.

Therefore various attempts were made to clarify raw Montan wax. It istrue that by means of the chemical retining methods roposed for thispurpose clear products can e obtained. However this result isaccompanied by an undesired chemical and, in comination therewith,physical alteration of the and in Germany September 18. 1927.

methyl glycollate, or ketones such as butanone. Mixtures of thesesolvents-may likewise be employed.

The invention therefore consists in extracting the resinsfrom the rawMontan wax, then dissolving the wax in the above-named solvents, and d1esting the solution with a decolorizing pow er, preferably withactivated carbon.

The resins may be extracted in the wellknown manner with any ap ropriatesolvent, for instance with benzene or enzine. Instead of the latter theabove-named solvents may be employed. In this case the bleaching opwaxso that the clear reaction product is deeratioumay' immediately followthe extracrived of certain other important properties t1on of the resinswithout the necessity of sepibr g characteristic features of rawMonaratmg the solvent retained by the extracted tan wax. wax.

This drawback is especially found when re- For car 'ng out our processwe may pro fining raw Montan wax by distillation, ceed as fol owswhereby the valuable wax esters are split up to a considerable degreeand moreover the output of refined wax is decreased. H v It has beenfurther imposed to extract raw Montan wax, prefera ly with the additionof a decolorizing powder such as bleachin earth, with solvents which donot or only di ficultly dissolve the oxyacids contained in the wax towhich acids the dark color is attributed in the first place. In fact bythis method cleared wax solutions are obtained. However ondistillinglofl the solvent from the wax the latter is at est, obtainedwith a li ht-brown color. The

bleaching efiect thus 0 tained is The Montanwax obtained by extractinbituminous coal with any suitable solvent an freedfrom resin by anyknown method is dissolved in one of the above-mentioned solvents withthe application of heat. The soldtion is'mixed with the decolorizingpowder not satisfactory for various applications. he consumfition f d loizing pow er 85 Now wehave found the surprising factthat may be reducedand theeifect o our'imthe relatively slight bleaching efiect obtained bythis method is due to the-presence of resinous constituents in the rawMontan 'wax and that consequentl incomparably clearer 4 products areobtaine by first extracting the resins from raw Montan wax by means ofdecolorizin powders such as bleachin earth and especia ly activatedcarbon, and t on digesting the extracted wax with solvents which do notor onl difliculty dissolve the oxyacids containe in the raw wax. Thispro 78 solvents, such as monohydric a cohols, or their esters or ethers,for

the

nt. The eficiencymf e several decolorants vanes.

(a' carbonactivsted by means of The best results are obtained a highlyactivated carbon, for instanee,-- Fearmstan ce ethel acetate and b0 p33, ester number 36.

zinc chloride) which for the sake of greater cheapness ma be replaced byless active decolorizing carlhons or earths.

The quantity of solvent required for refining the Montan wax dependsupon the solubility of the wax in the respective solvent and upon thequantity and efficiency of the decolorant employed.

Instead of the Montan wax freed from resins its constituents separatedin" the wellknown manner, for instance, the especially valuable andeasily clear-able wax esters, may be subjected to the bleachingoperation.

To obtain products of the most valuable properties the waxsolution,'after being diested with the decolorant and separated rom thelatter by filtering, may be cooled down and the thereby separated nearlywhite wax portions may be separately obtained.

This product equals or even surpasses carnauba 'wax in its chemical andphysical properties, for instance with respect to its capacity forabsorbing turpentine oil or with respect to its fusing point.

From the exhausted decolorizing carbon the retained Montan wax and theadsorbed and dankening constituents may be withdrawn by extraction withsuitable solvents,-

whereupon the carbon may be regenerated by known methods, forinstance,'by heating in a current of carbonic acid gas, and used again.

Examples fin at once, we may also proceed in such'a way that thesolution is first digested with only 40 parts of carboraflin, thenfiltered off, then again mixedand stirred with 35 parts of car borafiinand further treated as above. In this manner a uite pure,light-yellow'product is obtained. he dark portions of the waxremainingjin the activated carbon are separated by extraction withbenzene or the like. 78 parts of yellow Montan wax remain showing:fusing .point 85 (3., acid number 2. On the one band 100 parts of rawontan wax and on the other hand 100 pa ts of Montan wax well freed fromresin are dissolved in butanone under similar working conditions, andeach solution is mixed with 200 parts of a mixture of carboraflin (2parts) and decolorizing or fullers earth .(1 part).

The further treatment is the same as described in Exam le 1.' From theraw Montan wax a lightrown roduct is obtained; whereas the second prouct shows an almost pure white color.

3. The cthylacetate solution of the clarified wax obtained according toExample 1 after being filtered off from the decolorizing carbon iscooled down to 55 C: The precipltated wax is separated from the solutionby means of any suitable filtering device and the remaining solvent isremoved by heating. parts of an almost pure white product are obtained,the properties of wh1chfusing point- 88 0., acid number 9, ester number45arc the same as those of carnauba wax.

The solution remaining after separating the wax portions precipitated at55 C. is'

evaporated to dryness, whereby further 40 ,parts of a light-brown waxshowing: fusing constituents from raw Montan wax, digest:

ing the remaining wax, in presence of a solid adsorbent decolorizmgmaterial, with oxygenated organic solvents not easily dissolving'theoxy-acids contained in theraw Montan wax, separating the resulting waxsolu tion from the adsorbent, and separating the refined wax from thesolution.

2. Process for obtaining refined Montan wax which comprises extractingthe resinous constituents from raw Montan wax with oxygenated organicsolvents not easily dissolving the oxy-acids contained in the raw wax,igesting the remaining wax with a further quantity of the same solventsin presence of a solid adsorbent decolorizing material, se )arating theresulting wax solution from t e adsorbent, and separating the refinedwax. from the solution.

3. Process for obtaining refined Montan wax which comprises extractingthe resinous constituents from rawrMontan wax, stepwise digestin theremaining wax, in presence of a solid a sorbent decolorizing material,with oxygenated organic solvents not easily dissolv ng the ox'y-acidscontained in the raw Mpntan wax, separatin the resulting wax so utionfrom the adsor cut, and separating the'refined wax fromthe solution.

4. Process for obtaining refined Montan wax which comprises extractingthe resinous constituents from raw Montan wax with oxygenated organicsolvents not easily dissolving the. oxy-acids contained in the raw wax,stepwise digesting the remainin wax with a further quantity of the sameso vents in presence of a solid adsorbent decolorizing material,separating the resulting wax soluti on from the adsorbent andseparatingthe refinedwax from the solution.

5. Process for obtaining refined Montan wax which comprises extractingthe resinous constituents from raw Montan wax, digesting incounter-current the remaining wax, in presence of a solid adsorbentdecolorizing material, with oxygenated organic solvents not easilydissolving the oxy-acids contained in the raw Montan Wax, separatin theresulting wax solution from the adsor out, and separating the refinedwax from the solution.

6. Process for obtaining refined Montan wax which comprises extractingthe resinous constituents from raw Montan wax, digesting the remainingwax, in presence of a highly activated carbon, with oxygenated organicsolvents not easily dissolving the oxy-acids contained in the raw Montanwax, separating the resulting wax solution from the adsorbent, andseparating the refined wax from the solution.

7. Process for obtaining refined Montan wax which comprises extractingthe resinous constituents from raw Montan wax, digesting the remainingwax, in Presence of a carbon activated by means 0 zinc chloride withoxygenated organic solvents not easily dissolving the oxy-acidscontained in the raw Montan wax, separatin the resulting wax solutionfrom the adsor cut, and separatin the refined wax from the solution.

8. Process for obtaining refined Montan wax which comprises extractingthe resinous constituents from raw Montan wax, heating the remainingwax, in presence of a solid adsorbent decolorizing material, withoxygenated organic solvents not easily dissolving the o -acids containedin the raw Montan wax, tering off the resulting solution,

cooling the said solution, separating the precipitated wax from thesolution, and separating the wax from the latter.

9. Process for obtaining refined Montan tures.

FRITZ ZSCHOCH.

HERBERT, RODRIAN.

wax which comprises extracting the resinous constituents from raw.Montan wax, digesting the remaining wax, in presence of a solidadsorbent decolorizing material, with ethyl acetate, separating theresulting wax solution from the adsorbent, and separating the re-" finedwax from the resulting solution.

10. Process for obtaining refined Montan wax which comprises extractingthe resinous constituents from raw Montan wax, digesting the remainingwax, in presence of a solid adsorbent decolorizing material, withoxygenated organic solvents not easily dissolving the oxy-acidscontained in the raw Montan wax, separatin the resulting wax solutionfrom the adsor nt, extracting the exhausted decolorant with a solventcapable of dissolving the whole of the wax constituents containedtherein, and separating the refined wax and the extracted oxy-acids fromthe resulting solutions 11. Process for obtaining refined Montan waxwhich comprises extracting the resinous

